CN101903123A - Sintering furnace and method of making cutting tools - Google Patents
Sintering furnace and method of making cutting tools Download PDFInfo
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- CN101903123A CN101903123A CN2008801220158A CN200880122015A CN101903123A CN 101903123 A CN101903123 A CN 101903123A CN 2008801220158 A CN2008801220158 A CN 2008801220158A CN 200880122015 A CN200880122015 A CN 200880122015A CN 101903123 A CN101903123 A CN 101903123A
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- 238000005245 sintering Methods 0.000 title claims abstract description 119
- 238000005520 cutting process Methods 0.000 title claims abstract description 23
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 9
- 238000010438 heat treatment Methods 0.000 claims abstract description 104
- 238000000034 method Methods 0.000 claims abstract description 56
- 239000000843 powder Substances 0.000 claims abstract description 27
- 238000001816 cooling Methods 0.000 claims abstract description 18
- 238000009413 insulation Methods 0.000 claims abstract description 17
- 241000209094 Oryza Species 0.000 claims description 37
- 235000007164 Oryza sativa Nutrition 0.000 claims description 37
- 239000011159 matrix material Substances 0.000 claims description 37
- 235000009566 rice Nutrition 0.000 claims description 37
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 26
- 229910002804 graphite Inorganic materials 0.000 claims description 26
- 239000010439 graphite Substances 0.000 claims description 26
- 239000000463 material Substances 0.000 claims description 23
- 238000003825 pressing Methods 0.000 claims description 13
- 238000012544 monitoring process Methods 0.000 claims description 2
- 239000011230 binding agent Substances 0.000 abstract description 3
- 239000000758 substrate Substances 0.000 abstract description 2
- 238000007711 solidification Methods 0.000 abstract 1
- 230000008023 solidification Effects 0.000 abstract 1
- 230000008569 process Effects 0.000 description 20
- 229910045601 alloy Inorganic materials 0.000 description 15
- 239000000956 alloy Substances 0.000 description 15
- 229910017052 cobalt Inorganic materials 0.000 description 15
- 239000010941 cobalt Substances 0.000 description 15
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 15
- 239000012071 phase Substances 0.000 description 15
- 229910002091 carbon monoxide Inorganic materials 0.000 description 13
- 238000004458 analytical method Methods 0.000 description 8
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- 238000005516 engineering process Methods 0.000 description 6
- 238000012545 processing Methods 0.000 description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 5
- 239000011195 cermet Substances 0.000 description 5
- 239000000203 mixture Substances 0.000 description 5
- 239000002002 slurry Substances 0.000 description 4
- 229910000831 Steel Inorganic materials 0.000 description 3
- 230000008901 benefit Effects 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 239000010959 steel Substances 0.000 description 3
- 238000005255 carburizing Methods 0.000 description 2
- 238000005056 compaction Methods 0.000 description 2
- 230000002950 deficient Effects 0.000 description 2
- 238000013461 design Methods 0.000 description 2
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- 238000001462 microwave scanning near-field microscopy Methods 0.000 description 2
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- 229910052758 niobium Inorganic materials 0.000 description 2
- 229910052715 tantalum Inorganic materials 0.000 description 2
- 229910052721 tungsten Inorganic materials 0.000 description 2
- 229910001069 Ti alloy Inorganic materials 0.000 description 1
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- 230000001070 adhesive effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000011088 calibration curve Methods 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
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- 239000011261 inert gas Substances 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000314 lubricant Substances 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 238000003801 milling Methods 0.000 description 1
- 229910052750 molybdenum Inorganic materials 0.000 description 1
- 150000004767 nitrides Chemical class 0.000 description 1
- 238000004663 powder metallurgy Methods 0.000 description 1
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- UONOETXJSWQNOL-UHFFFAOYSA-N tungsten carbide Chemical compound [W+]#[C-] UONOETXJSWQNOL-UHFFFAOYSA-N 0.000 description 1
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- 229910052726 zirconium Inorganic materials 0.000 description 1
Images
Classifications
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B17/00—Furnaces of a kind not covered by any preceding group
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/003—Apparatus, e.g. furnaces
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F3/00—Manufacture of workpieces or articles from metallic powder characterised by the manner of compacting or sintering; Apparatus specially adapted therefor ; Presses and furnaces
- B22F3/10—Sintering only
- B22F3/1017—Multiple heating or additional steps
- B22F3/1028—Controlled cooling
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27B—FURNACES, KILNS, OVENS, OR RETORTS IN GENERAL; OPEN SINTERING OR LIKE APPARATUS
- F27B5/00—Muffle furnaces; Retort furnaces; Other furnaces in which the charge is held completely isolated
- F27B5/06—Details, accessories, or equipment peculiar to furnaces of these types
- F27B5/14—Arrangements of heating devices
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F27—FURNACES; KILNS; OVENS; RETORTS
- F27D—DETAILS OR ACCESSORIES OF FURNACES, KILNS, OVENS, OR RETORTS, IN SO FAR AS THEY ARE OF KINDS OCCURRING IN MORE THAN ONE KIND OF FURNACE
- F27D21/00—Arrangements of monitoring devices; Arrangements of safety devices
- F27D21/0014—Devices for monitoring temperature
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F5/00—Manufacture of workpieces or articles from metallic powder characterised by the special shape of the product
- B22F2005/001—Cutting tools, earth boring or grinding tool other than table ware
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2203/00—Controlling
- B22F2203/11—Controlling temperature, temperature profile
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F2999/00—Aspects linked to processes or compositions used in powder metallurgy
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Manufacturing & Machinery (AREA)
- Powder Metallurgy (AREA)
Abstract
The present invention relates to a method of making cutting tools comprising a substrate having a hard phase and a binder phase, the method comprising forming green powder compacts using powder metallurgical techniques, charging the green powder compacts, placed on one or several trays, in a furnace and sintering the green powder compacts wherein the furnace comprises an insulation package (9), at least three individually controlled heating elements located inside the insulation package (9) including a vertical heating element (5), an upper horizontal heating element (6) arranged in an upper part of the furnace, and a lower horizontal heating element (7) arranged in a lower part of the furnace, wherein operating the at least three heating elements such that an average controlled cooling rate from a sintering temperature down to at least a solidification temperature of the binder phase is 0.1-4.0 DEG C/min, and a sintering furnace operable to obtain a controlled cooling rate.
Description
Technical field
The present invention relates to a kind of manufacturing and be used for method such as the cutting tool of the machine operations of milling, boring and turning.
Background technology
The alloy based on tungsten carbide that is commonly referred to as carbide alloy is used for far-ranging application; The most important thing is as the material that is used for cutting tool.In this was used, alloy generally comprised the cobalt binder phase, and can comprise a spot of one or more IVa, Va and VIa family element usually.Another important materials group that is used for the cutting tool application is based on the alloy of titanium carbonitride, is commonly referred to cermet.They comprise the metal bonding phase of cobalt and/or nickel usually, and comprise the modal carbide and/or the nitride of one or more IVa, Va and VIa family element.
For example carbide alloy or the ceramic-metallic matrix that is used for cutting tool utilize powder metallurgy process production.Usually, this is included in the slurry and mixes/mill powder that forms the bonding phase and the powder that forms the hard component, the injected subsequently powder of preparing compacting (RTP) that is dried to of slurry, the RTP powder compaction is become the compacting green compact, and the compacting green sintering is become fine and close carbide alloy or cermet matrix.
The size and dimension of matrix is crucial for the performance of cutter, but can depart from nominal value because of the variation in the above-mentioned production stage usually.The deviation that is caused by sintering depends primarily on forming of the type of sintering furnace and design, position, sintering process and the matrix of compacting green compact in the sintering furnace batch of material.One type of the distortion relevant with sintering is matrix distortion (warpage), this is because uncontrolled carburizing or decarburizing reaction between matrix and their environment (being support member or the gas atmosphere in the sintering furnace) cause, as U.S. Patent No. 5,151,247.The sintering warpage of another known type is relevant with the gravity effect.Main for alloy with higher metal adhesive content and bigger body, the distortion of these types is problematic.When for example producing cutting tool insert, this effect is little, and can be compensated in the compacting Tool Design.
Utilize the grinding operation behind the sintering to correct dimensional discrepancy traditionally, but should operation more and more expensive along with the size of defective.For the cutter that is sintered directly into final size and shape, the cutting tool of promptly alleged direct compacting, deformation energy causes orientation problem.An example is when the cutting tool insert that will directly suppress is installed in the cutter retainer, and wherein dimensional defects can cause the relatively poor tolerance of uncertain abrasional behavior and surface of the work.
In U.S. Patent No. 5,151, in 247, disclose the inert gas that in the liquid-phase sintering process, utilizes high pressure and alleviated the carburizing mentioned or the method for decarburizing reaction.In U.S. Patent No. 5,993, in 970, disclose and selected to be used for graphite and support the suitable coating energy minimization matrix of pallet and the reaction between the support member.
EP1,468,764 disclose the method for the dimensional discrepancy that is used to reduce cemented carbide body, and this method is by being placed on sintered plate on an orientation main body after compacting and carrying out the dimensional discrepancy that the isotropism sintering process reduces cemented carbide body.Thereby the size distortion that is caused by sintering process will compensate the distortion that is caused by pressing operation.
Summary of the invention
The purpose of this invention is to provide the method that is used for Production Example such as carbide alloy or ceramic-metallic cutting tool matrix, described method reduces the needs to the grinding operation behind the sintering.
Find surprisingly, for example can reduce greatly by carrying out sintering process under given conditions that the size of carbide alloy and ceramic-metallic cutting tool matrix departs from nominal value.Find surprisingly that also undiscovered bonding phase content changes before significantly having reduced under these sintering conditions, wherein the different piece of sintering matrix material departs from nominal composition.Therefore, can go out on all cutting edges, to have near cutting tool nominal and the size material property of expecting by made according to the method for the present invention.
Description of drawings
Fig. 1 has shown the section according to exemplary sintering furnace of the present invention.
Fig. 2 has shown according to two of exemplary sintering furnace of the present invention different side views.
Fig. 3 schematically illustrates sintering pallet (left side) with cutting tool matrix and the matrix with side S1-S4 (right side).
Fig. 4 schematically illustrates the cutting tool insert that is divided into part B1-B4.
The specific embodiment
According to the present invention, the method of making cutting tool is provided, described cutting tool comprises and comprises hard mutually and bond mutually for example carbide alloy or ceramic-metallic matrix, described method comprises: utilize PM technique to form the powder pressing green compact, the powder pressing green compact that are placed on one or several pallets are installed in the stove, and the powder pressing green sintering become preferred dense substrate, wherein said stove comprises thermal insulation layer 9, be positioned at least three independent controlled heating element heaters of thermal insulation layer 9, described at least three independent controlled heating element heaters comprise the vertical heating element heater 5 that is fit to surround at least in part or several pallets, the lower horizontal heating element heater 7 that is arranged in the upper level heating element heater 6 on stove top and is arranged in the stove bottom, wherein, operate described at least three heating element heaters, make that the average controlled cooldown rate that drops to the setting temperature of the phase that bonds at least from sintering temperature is 0.1 ℃/minute-4.0 ℃/minute, be preferably 1.5 ℃/minute-2.5 ℃/minute.
The present invention also provides sintering furnace, comprise thermal insulation layer 9, be positioned at least three independent controlled heating element heaters of thermal insulation layer 9, described at least three independent controlled heating element heaters comprise and are fit to surround at least in part one or the vertical heating element heater 5 of several pallets, the lower horizontal heating element heater 7 that is arranged in the upper level heating element heater 6 on stove top and is arranged in the stove bottom, wherein, described at least three heating element heaters can be operated and obtain 0.1 ℃/minute-4.0 ℃/minute, be preferably 1.5 ℃/minute-2.5 ℃/minute average controlled cooldown rate.
In one embodiment, described method comprises: the powder and formation bonding powder mutually that mix in slurry and mill and form the hard component, produce the powder of preparing compacting by for example jet drying cause slurry, to prepare the powder compaction powdered compacting green compact of compacting, and the powder pressing green sintering is become fine and close carbide alloy or cermet matrix.
In one embodiment, carry out sintering in the vertical column stove (Fig. 1 and Fig. 2) of one or several feature in having following details.Vertically the column heat size is received one pile of circular graphite pallet 1, and for example carbide alloy or ceramic-metallic powder pressing green compact are placed on the pallet.Do not needing to make pressed compact aligning or rotation on pallet specially before the sintering and in sintering process.Sintering furnace comprises: the steel bushing 8 of outside basic column; The thermal insulation layer 9 of basic column, described thermal insulation layer 9 is preferably made by graphite, is positioned at steel bushing 8 inside of column, and described thermal insulation layer 9 is made up of column insulating portion 10, top thermal insulating disc 11 and bottom thermal insulating disc 12; At least three independent controlled heating element heaters, described at least three independent controlled heating element heaters can be made by graphite, be positioned at thermal insulation layer 9, it comprises the vertical column heating element heater 5 that is arranged in the column insulating portion 10, the upper level heating element heater 6 below stove top is arranged in top thermal insulating disc 11 and at the lower horizontal heating element heater 7 of stove lower disposed above bottom thermal insulating disc 12.Described at least one vertical column heating element heater 5 surrounds this pile pallet, make hot-fluid pallet in the radial direction the symmetry.Vertically the scope of the diameter D of heating element heater is 150mm to 600mm, and is preferably 400mm to 460mm.Vertically the scope of the height H of heating element heater is 50mm to 1000mm, and is preferably 530mm to 630mm.And upper level heating element heater 6 is positioned at the top pallet top, and lower horizontal heating element heater 7 is positioned at the bottom tray below.Upper level heating element heater 6 and lower horizontal heating element heater 7 development length in the horizontal direction are less than the diameter D of vertical column heating element heater 5.
In addition, in a preferred embodiment, at least three thermocouples independently, thermocouple 13, top thermocouple 14 and bottom thermocouple 15 in the middle of comprising, near vertical column heating element heater 5, upper level heating element heater 6 and lower horizontal heating element heater 7 location, be used for monitoring the temperature of stove and control heating region respectively.
An extra thermocouple 16 can be positioned the centre of the batch material (batch) of material very close to be sintered.This thermocouple specifically provides important technique information in unsticking (debinding) and coagulation step, wherein the reaction heat energy from the bond matrix phase is monitored to.
In addition, in sintering process, specifically drop to the controlled cooling procedure of setting temperature at least from sintering temperature, described extra thermocouple 16 and the difference between the middle thermocouple 13 can not allow to surpass described setup parameter alternatively with the setup parameter in the action control system in technical process.The purpose of the adjusting of the type in control system is to minimize the thermograde of radial direction on the pallet.
The diameter range of sintering pallet is preferably 0.25*D to 0.99*D, 0.55*D to 0.80*D more preferably, and most preferably be 0.65*D to 0.70*D, wherein D is the diameter of vertical column heating element heater 5.The altitude range of this pile pallet is preferably 0.01*H to 1.0*H, 0.85*H to 0.95*H more preferably, and wherein H is the height of vertical column heating element heater 5.
In a preferred embodiment, thermal insulation layer 9 surrounds described at least three heating element heaters, and is made by graphite, and has following size.The inside diameter ranges of column insulating portion 10 is 1.04*D to 2.0*D, be preferably 1.15*D to 1.35*D, wherein D is the diameter of vertical column heating element heater 5, and the height of column insulating portion 10 is 1.1*H to 2.5*H, be preferably 1.7*H to 2.1*H, wherein H is the height of vertical column heating element heater 5.The thickness range of column insulating portion 10 is 20mm to 60mm, is preferably 35mm-45mm.The thickness range of top thermal insulating disc 11 and bottom thermal insulating disc 12 is 35mm-85mm, is preferably 55mm-65mm.The outside of stove, promptly basically column steel bushing 8 by water cooling.
In another embodiment, this pile pallet is enclosed in the column graphite rice steamer of being made up of three parts (retort), and described three parts are rice steamer tube 2, rice steamer top board 3 and rice steamer base plate 4.Described rice steamer is between described at least three heating element heaters 5,6,7 and this pile pallet 1, to improve the control of the thermograde in the stove in the cooling procedure.The internal diameter of rice steamer tube 2 is 0.30*D to 0.99*D, is preferably 0.70*D to 0.78*D, and wherein D is the diameter of vertical column heating element heater 5.The graphite rice steamer is usually by rice steamer top board 3 and rice steamer base plate 4 closures, and as shown in Figure 2, but plate can be opened, for example to improve quick cooling procedure.The wall thickness of rice steamer tube 2, rice steamer top board 3 and rice steamer base plate 4 is 5mm to 20mm, is preferably 7mm to 8mm.
The size of thermal insulation layer and rice steamer and material property are combined into feasible, in the situation of empty stove, promptly in the situation without any the graphite pallet, average nature (freely) cooldown rate drop to 1200 ℃ temperature range from 1400 ℃ is 9 ℃/minute to 14 ℃/minute a scope.Cooling velocity is by the mean temperature decision from middle thermocouple 13, top thermocouple 14 and bottom thermocouple 15.
The first that the sintering circulation has the temperature range that is in 20 ℃-450 ℃, it is the unsticking step, purpose is to remove the organic lubricant of compacting green compact.Be that composition, the reach that depends on matrix is the heating in vacuum step of 1350 ℃-1550 ℃ sintering temperature after this step.Third step (actual sintered) carries out under the gross pressure between 0.001 millibar to 900 millibars.When sintering process finished, scope was introduced alternatively in 20 crust to the high pressure gas physical efficiency between 100 crust, to avoid undesired defective and to improve the density of material.In these three processing steps, the pith that charging is heated is produced by lower horizontal heating element heater 7, so that in the vertical direction is realized good temperature homogeneity in whole charging.
It after sintering step the controlled cooling step that drops to the setting temperature of the phase that bonds at least the batch of material from sintering temperature.The scope of average controlled cooldown rate is 0.1 ℃/minute to 4.0 ℃/minute, is preferably 1.5 ℃/minute to 2.5 ℃/minute, the thermograde of each matrix when solidifying to minimize.Controlled cooldown rate by thermocouple 13, top thermocouple 14 and bottom thermocouple 15 in the middle of comprising at least three independently thermocouple measure, realize by applying from the power of described at least three the independent controlled heating element heaters that comprise vertical column heating element heater 5, upper level heating element heater 6 and lower horizontal heating element heater 7.Total power profile between described at least three heating element heaters is influential to the thermograde of radial direction on the pallet.Surpass 70% general power by applying, can reduce the thermograde of radial direction on the pallet by vertical column heating element heater 5.When applying 100% power, thereby when in controlled cooling step, cutting off upper level heating element heater 6 and lower horizontal heating element heater 7, realized another improvement by vertical column heating element heater 5.
Solidifying of the bonding phase of matrix can be supervised side by middle thermocouple 16, describedly is solidified as exothermic reaction, and is crucial to producing dimensional discrepancy.For middle thermocouple 16 being used and keeping radial symmetric, need have the sintering pallet of centre bore in the middle of batch of material.After all bondings in batch of material have all been solidified mutually (this can observe from middle thermocouple 16), quick cooling step can be begun immediately,, and the material and the dimensional performance of matrix can be influenced sharply so that reduce total sintering process time.
Described sintering furnace and technology is main to be used for carbide alloy and the cermet grade that sintering has the higher bonding phase content of the Co that is higher than 13 volume % and/or Ni.For grade with this component, be to compare significantly with the normal sintering method, deviation reduced in size and the reducing benefit that phase content changes that bonds.The present invention can also be used to be lower than the grade of specific bonding phase content restriction, but contrasting the normal sintering method observes more unconspicuous raising.
The present invention can be applied to have the grade of Com/Co, promptly in being used for all tolerance bands of cutting tool product, and magnetic cobalt wt%/Co wt% in carbide alloy or cermet.But, when Com/Co is lower than 0.95, compare with normal sintering, it is more remarkable to reduce dimensional discrepancy and the reducing benefit that phase content changes that bonds.
Described sintering furnace and technology are used to produce the cutting tool with all types of sizes and geometry.Yet, need dissimilar measurements to be identified for the feature of different geometries such as the dimensional discrepancy of square, rhombus, circle, triangle etc.Because the distortion relevant with sintering depends on blade size, have more advantages on the bigger blade so purposes of the present invention is found in, thereby reduce absolute deformation significantly.
The present invention can set forth by the batch of material of SNMM-15 compacting green compact of grade that sintering has the bonding phase composition of the Co that surpasses 13 volume % and/or Ni.Because the size distortion of the SNMM of square configuration and bonding phase change are measured easily, so select the SNMM of described geometry.Utilization is carried out sintering according to stove of the present invention and sintering process.After sintering, according to the position of Fig. 3 16 matrixes (No. 1 to No. 16) are taken a sample from a pallet.Measure four edge lengths S1 to S4 (Fig. 3) of each body, and the edge lengths between the calculating relative edge is poor: d
24=(S2-S4) and d
31=(S3-S1).Utilization is according to sintering furnace of the present invention and technology, the d between 16 matrixes
24And d
31Variation less than ± 25 μ m.For the bonding phase change is shown, No. 1, matrix and No. 9 (Fig. 3) are cut into 9 parts, referring to Fig. 4.The use chemical analysis is measured the Co content on the matrix.Utilization is according to sintering furnace of the present invention and technology, and the high cobalt content of four part B1-B4 and the difference between the minimum cobalt content are less than 0.20wt% in the matrix No. 1 and No. 9.
Example 1
By wet-milling WC, Co, TaC and Ta
0.8Nb
0.2C prepares nominal and forms (wt%) mixture of powders for the commercially available carbide alloy grade of 11.50%Co, 81.61%W, 1.17%Ta, 0.28%Nb.Powderject is dry and be pressed into the SNMM-15 compacting green compact of the square geometry of the nominal sintering edge lengths with 15mm.Powder property and compacting circulation are selected such that the variation minimum of powder density in the body, thereby reduce the warpage that caused by powder and pressing process.After compacting,, the compacting green compact are placed on the circular sintering pallet that diameter is 290mm according to common operation.About 72 compacting green compact are placed on each sintering pallet, referring to Fig. 3.Do not use the concrete rotation or the aligning of the compacting green compact on the pallet.
Example 2 (the present invention)
In vertical column stove, at one pile of pressed compact of the compacting of sintering example 1 on 50 height that form 600mm, the sintering pallet that diameter is 290mm altogether.Material pallet is for waiting graphite of static pressure compacting.The diameter of the column heating element heater of stove is 430mm, highly is 580mm, and thickness is 15mm.At top and bottom heating element heater is arranged also, thickness all is 15mm.Between heating element heater and this pile graphite pallet the graphite rice steamer is arranged, its top board and base plate are closed in whole technical process.The internal diameter of column rice steamer is 310mm, highly is 580mm, and thickness is 7.5mm.The top board of rice steamer and the thickness of base plate also are 7.5mm.The internal diameter that is positioned the column insulating portion of rice steamer outside is 540mm, highly is 1150mm.The thickness of column insulating portion is 40mm, and the thickness of top section and base section is 80mm.
At first in 20 ℃-450 ℃ temperature range, make compacting green compact unsticking.Be 60 minutes vacuum step after this step, temperature is elevated to 1410 ℃ of sintering temperatures in vacuum step.Under 40 millibars gross pressure, carry out 60 minutes sintering 1410 ℃ of utilizations by the atmosphere that Ar and CO form.In these processing steps, the power between the heating element heater distributes and is about: shaped element 55%, base member 25% and crown member 20%.
After sintering step, utilizing atmosphere speed with 2 ℃/minute under 40 millibars gross pressure of forming by Ar and CO to carry out controlled cooling step between 1410 ℃ and 1200 ℃.In this step, bottom and top heating element heater are cut off, thereby all heat is all produced by the column heating element heater.After sintering, from the sintering pallet to No. 1 to No. 16 sampling of matrix of the centre that is positioned at charging, for use in analysis, referring to Fig. 3.These matrixes are called as sample A.
Example 3 (the present invention)
In vertical column stove, at one pile of pressed compact of the compacting of sintering example 1 on 50 height that form 600mm, the sintering pallet that diameter is 290mm altogether.Material pallet is for waiting graphite of static pressure compacting.The diameter of the column heating element heater of stove is 430mm, highly is 580mm, and thickness is 15mm.At top and bottom heating element heater is arranged also, thickness all is 15mm.Between heating element heater and this pile graphite pallet the graphite rice steamer is arranged, its top board and base plate are closed in whole technical process.The internal diameter of column rice steamer is 310mm, highly is 580mm, and thickness is 7.5mm.The top board of rice steamer and the thickness of base plate also are 7.5mm.The internal diameter that is positioned the column insulating portion of rice steamer outside is 540mm, highly is 1150mm.The thickness of column insulating portion is 40mm, and the thickness of top section and base section is 80mm.
At first in 20 ℃-450 ℃ temperature range, make compacting green compact unsticking.Be 60 minutes vacuum step after this step, temperature is elevated to 1410 ℃ of sintering temperatures in vacuum step.Under 40 millibars gross pressure, carry out 60 minutes sintering 1410 ℃ of utilizations by the atmosphere that Ar and CO form.In these processing steps, the power between the heating element heater distributes and is about: shaped element 55%, base member 25% and crown member 20%.
After sintering step, utilizing atmosphere speed with 2 ℃/minute under 40 millibars gross pressure of forming by Ar and CO to carry out controlled cooling step between 1410 ℃ and 1200 ℃.In this step, the power between the heating element heater is distributed as: shaped element 70%, base member 25% and crown member 5%.After sintering, from of matrix No. 1 to No. 16 sampling of sintering pallet, for use in analysis, referring to Fig. 3 to the centre that is positioned at charging.These matrixes are called as sample B.
Example 4 (the present invention)
In vertical column stove, at one pile of pressed compact of the compacting of sintering example 1 on 50 height that form 600mm, the sintering pallet that diameter is 290mm altogether.Material pallet is for waiting graphite of static pressure compacting.The diameter of the column heating element heater of stove is 430mm, highly is 580mm, and thickness is 15mm.At top and bottom heating element heater is arranged also, thickness all is 15mm.The internal diameter of column insulating portion is 540mm, highly is 1150mm.The thickness of column insulating portion is 40mm, and the thickness of top section and base section is 80mm.
At first in 20 ℃-450 ℃ temperature range, make compacting green compact unsticking.Be 60 minutes vacuum step after this step, temperature is elevated to 1410 ℃ of sintering temperatures in vacuum step.60 minutes sintering that the atmosphere of being made up of Ar and CO 1410 ℃ of utilizations is carried out under 40 millibars gross pressure.In these processing steps, the power between the heating element heater distributes and is about: shaped element 55%, base member 25% and crown member 20%.
After sintering step, utilizing atmosphere speed with 2 ℃/minute under 40 millibars gross pressure of forming by Ar and CO to carry out controlled cooling step between 1410 ℃ and 1200 ℃.In this step, the power between the heating element heater is distributed as: shaped element 25%, base member 35% and crown member 40%.After sintering, from the sintering pallet to No. 1 to No. 16 sampling of matrix of the centre that is positioned at charging, for use in analysis, referring to Fig. 3.These matrixes are called as sample C.
Example 5 (the present invention)
In vertical column stove, at one pile of pressed compact of the compacting of sintering example 1 on 50 height that form 600mm, the sintering pallet that diameter is 290mm altogether.Material pallet is for waiting graphite of static pressure compacting.The diameter of the column heating element heater of stove is 430mm, highly is 580mm, and thickness is 15mm.At top and bottom heating element heater is arranged also, thickness all is 15mm.Between heating element heater and this pile graphite pallet the graphite rice steamer is arranged, its top board and base plate are closed in whole technical process.The internal diameter of column rice steamer is 310mm, highly is 580mm, and thickness is 7.5mm.The top board of rice steamer and the thickness of base plate also are 7.5mm.The internal diameter that is positioned the column insulating portion of rice steamer outside is 540mm, highly is 1150mm.The thickness of column insulating portion is 40mm, and the thickness of top section and base section is 80mm.
At first in 20 ℃-450 ℃ temperature range, make compacting green compact unsticking.Be 60 minutes vacuum step after this step, temperature is elevated to 1410 ℃ of sintering temperatures in vacuum step.Under 40 millibars gross pressure, carry out 60 minutes sintering 1410 ℃ of utilizations by the atmosphere that Ar and CO form.In these processing steps, the power between the heating element heater distributes and is about: shaped element 55%, base member 25% and crown member 20%.
After sintering step, utilizing atmosphere speed with 4 ℃/minute under 40 millibars gross pressure of forming by Ar and CO to carry out controlled cooling step between 1410 ℃ and 1200 ℃.In this step, the power between the heating element heater is distributed as: shaped element 25%, base member 35% and crown member 40%.After sintering, from the sintering pallet to No. 1 to No. 16 sampling of matrix of the centre that is positioned at charging, for use in analysis, referring to Fig. 3.These matrixes are called as sample D.
Example 6 (contrast)
In vertical column stove, at one pile of pressed compact of the compacting of sintering example 1 on 50 height that form 600mm, the sintering pallet that diameter is 290mm altogether.Material pallet is for waiting graphite of static pressure compacting.The diameter of the column heating element heater of stove is 430mm, highly is 580mm, and thickness is 15mm.At top and bottom heating element heater is arranged also, thickness all is 15mm.The internal diameter of column insulating portion is 540mm, highly is 1150mm.The thickness of column insulating portion is 40mm, and the thickness of top section and base section is 80mm.
At first in 20 ℃-450 ℃ temperature range, make compacting green compact unsticking.Be 60 minutes vacuum step after this step, temperature is elevated to 1410 ℃ of sintering temperatures in vacuum step.Under 40 millibars gross pressure, carry out 60 minutes sintering 1410 ℃ of utilizations by the atmosphere that Ar and CO form.In these processing steps, the power between the heating element heater distributes and is about: shaped element 55%, base member 25% and crown member 20%.
After sintering step, the Mean Speed that allows to feed with 9 ℃/minute naturally cools to 1200 ℃ from sintering temperature.After sintering, from of matrix No. 1 to No. 16 sampling of sintering pallet, for use in analysis, referring to Fig. 3 to the centre that is positioned at charging.These matrixes are called as sample E.
Example 7
From whole 16 matrixes of sample A-E, use coordinate measuring machine to measure the edge lengths of limit 1,2,3 and 4 (S1-S4), referring to Fig. 4.According to d
24=(S2-S4) and d
31=(S3-S1) calculate the poor d of the edge lengths between the relative edge
24And d
31The variation of the edge lengths on the sintering pallet can be expressed as d
24And d
31Maximum and the scope between the minimum of a value:
Δ d
24 maximums-minimum=maximum (d
24)-minimum (d
24)
Δ d
31 maximums-minimum=maximum (d
31)-minimum (d
31)
Table 1 has shown the Δ d of the sample A-E that is obtained
24 maximums-minimumValue and Δ d
31 maximums-minimumValue.Because these values corresponding to the dimensional discrepancy that is caused by sintering process and stove, so wish to make their minimums, in contrast to sample E, sample A-D has realized making their minimums.
Table 1
| Sample | Δd 24 maximums-minimum | Δd 31 maximums-minimum |
| A | 16 | 33 |
| B | 28 | 32 |
| C | 33 | 39 |
| D | 26 | 47 |
| E | 70 | 66 |
After dimensional measurement, will cut into 9 parts according to Fig. 5 from No. 1, the matrix of sample A, D and E and No. 9.Use X-ray fluorescence spectra to come the cobalt content of determining section B1-B4.This method has been used the calibration curve of cobalt content scope as 0.98%-25%, and has considered the influence of other elements of existence usually in carbide alloy, such as the influence of element ti, Cr, Fe, Ni, Nb, Mo, Ta, W, Zr, V and Mn.From three duplicate measurements to each sample, the error of this method is confirmed as ± 0.02%Co.
Use the high cobalt content of four part B1-B4 in the matrix and the difference between the minimum cobalt content quantizes cobalt content in the matrix as variable variation.In table 2, shown that the cobalt content of sample A, D and E changes.E compares with sample, and the cobalt content of sample A and D changes obviously less.In the matrix Co change relevant with position on the sintering pallet, make matrix towards the cobalt content of the directed part of pallet periphery than partial C o content height towards the middle orientation of pallet.
Table 2
| Sample | Cobalt content changes, No. 1, matrix (wt%) | Cobalt content changes, No. 9, matrix (wt%) |
| A | 0.12 | 0.16 |
| D | 0.18 | 0.11 |
| E | 0.29 | 0.36 |
Example 8
Utilize and the make powder batch of material of compacting green compact of identical component described in the example 1 and technology.After pressing process, the powder pressing green compact are placed on the circular sintering pallet that diameter is 290mm according to common operation.About 72 powder pressing green compact on each sintering pallet, have been placed, referring to Fig. 3.
Example 9 (the present invention)
In vertical column stove, at one pile of pressed compact of the compacting of sintering example 8 on 50 height that form 600mm, the sintering pallet that diameter is 290mm altogether.Material pallet is for waiting graphite of static pressure compacting.The diameter of the column heating element heater of stove is 430mm, highly is 580mm, and thickness is 15mm.At top and bottom heating element heater is arranged also, thickness all is 15mm.Between heating element heater and this pile graphite pallet the graphite rice steamer is arranged, its top board and base plate are closed in whole technical process.The internal diameter of column rice steamer is 310mm, highly is 580mm, and thickness is 7.5mm.The top board of rice steamer and the thickness of base plate also are 7.5mm.The internal diameter that is positioned the column insulating portion of rice steamer outside is 540mm, highly is 1150mm.The thickness of column insulating portion is 40mm, and the thickness of top section and base section is 80mm.
At first in 20 ℃-450 ℃ temperature range, make compacting green compact unsticking.Be 60 minutes vacuum step after this step, temperature is elevated to 1410 ℃ of sintering temperatures in vacuum step.60 minutes sintering that the atmosphere of being made up of Ar and CO 1410 ℃ of utilizations is carried out under 40 millibars gross pressure.
After sintering step, utilizing atmosphere speed with 2 ℃/minute under 40 millibars gross pressure of forming by Ar and CO to carry out controlled cooling step between 1410 ℃ and 1200 ℃.After sintering, from the sintering pallet to No. 1 to No. 16 sampling of matrix of the centre that is positioned at charging, for use in analysis, referring to Fig. 3.These matrixes are called as sample F.
Example 10 (the present invention)
In vertical column stove, at one pile of pressed compact of the compacting of sintering example 8 on 50 height that form 600mm, the sintering pallet that diameter is 290mm altogether.Material pallet is for waiting graphite of static pressure compacting.The diameter of the column heating element heater of stove is 430mm, highly is 580mm, and thickness is 15mm.At top and bottom heating element heater is arranged also, thickness all is 15mm.Between heating element heater and this pile graphite pallet the graphite rice steamer is arranged, its top board and base plate are closed in whole technical process.The internal diameter of column rice steamer is 310mm, highly is 580mm, and thickness is 7.5mm.The top board of rice steamer and the thickness of base plate also are 7.5mm.The internal diameter that is positioned the column insulating portion of rice steamer outside is 530mm, highly is 1150mm.The thickness of column insulating portion is 52mm, and the thickness of top section is 140mm, and the thickness of base section is 98mm.
At first in 20 ℃-450 ℃ temperature range, make compacting green compact unsticking.Be 60 minutes vacuum step after this step, temperature is elevated to 1410 ℃ of sintering temperatures in vacuum step.60 minutes sintering that the atmosphere of being made up of Ar and CO 1410 ℃ of utilizations is carried out under 40 millibars gross pressure.
After sintering step, utilizing atmosphere speed with 2 ℃/minute under 40 millibars gross pressure of forming by Ar and CO to carry out controlled cooling step between 1410 ℃ and 1200 ℃.After sintering, from of matrix No. 1 to No. 16 sampling of sintering pallet, for use in analysis, referring to Fig. 3 to the centre that is positioned at charging.These matrixes are called as sample G.
Example 11
On whole 16 matrixes from sample F and G, measure the edge lengths of limit 1,2,3 and 4 (S1-S4), and according to d
24=(S2-S4) and d
31=(S3-S1) calculate the poor d of the edge lengths between the relative edge
24And d
31The variation of the edge lengths on the sintering pallet can be expressed as d
24And d
31Maximum and the scope between the minimum of a value:
Δ d
24 maximums-minimum=maximum (d
24)-minimum (d
24)
Δ d
31 maximums-minimum=maximum (d
31)-minimum (d
31)
Table 3 has shown the sample F that obtained and the Δ d of G
24 maximums-minimumValue and Δ d
31 maximums-minimumValue.
Table 3
| Sample | Δd 24 maximums-minimum | Δd 31 maximums-minimum |
| F | 30 | 24 |
| G | 43 | 47 |
Claims (14)
1. method of making cutting tool, described cutting tool comprises and comprises hard mutually and mutually the matrix of boning, described method comprises: utilize PM technique to form the powder pressing green compact, the described powder pressing green compact that are placed on one or several pallets are installed in the stove, and the described powder pressing green compact of sintering, wherein, described stove comprises thermal insulation layer (9), be positioned at least three independent controlled heating element heaters of described thermal insulation layer (9), described at least three independent controlled heating element heaters comprise vertical heating element heater (5), the lower horizontal heating element heater (7) that is arranged in the upper level heating element heater (6) on described stove top and is arranged in described stove bottom, it is characterized in that, operate described at least three heating element heaters, make that the average controlled cooldown rate that drops to the setting temperature of described at least bonding phase from sintering temperature is 0.1 ℃/minute-4.0 ℃/minute.
2. the method for claim 1 is characterized in that, the average controlled cooldown rate that drops to described at least setting temperature from described sintering temperature is 1.5 ℃/minute-2.5 ℃/minute.
3. as the described method of claim 1-2, it is characterized in that described vertical heating element heater (5) surrounds described one or several pallets at least in part.
4. as the described method of claim 1-3, it is characterized in that described stove is vertical column stove.
5. the described method of each claim as described above, it is characterized in that, described vertical heating element heater is a vertical column heating element heater (5), the scope of the diameter D of described vertical column heating element heater (5) is 150mm to 600mm, and be preferably 400mm to 460mm, and the scope of the height H of described vertical heating element heater is 50mm to 1000mm, and is preferably 530mm to 630mm.
6. the described method of each claim as described above is characterized in that described thermal insulation layer (9) is made up of column insulating portion (10), top thermal insulating disc (11) and bottom thermal insulating disc (12).
7. method as claimed in claim 6, it is characterized in that the thickness range of described column insulating portion (10) is 20mm to 60mm, is preferably 35mm to 45mm, and the thickness range of described top thermal insulating disc (11) and described bottom thermal insulating disc (12) is 35mm to 85mm, is preferably 55mm to 65mm.
8. as the described method of claim 6-7, it is characterized in that, the inside diameter ranges of described column insulating portion (10) is 1.04*D to 2.0*D, be preferably 1.15*D to 1.35*D, wherein D is the diameter of described vertical column heating element heater (5), and the height of described column insulating portion (10) is 1.1*H to 2.5*H, is preferably 1.7*H to 2.1*H, and wherein H is the height of described vertical column heating element heater (5).
9. the described method of each claim as described above, it is characterized in that, described stove and accessory has at least three independently thermocouples, comprises middle thermocouple (13), top thermocouple (14) and the bottom thermocouple (15) of locating near described vertical column heating element heater (5), described upper level heating element heater (6) and described lower horizontal heating element heater (7) respectively.
10. the described method of each claim as described above is characterized in that, the cooling procedure of the described setting temperature that drops to described at least bonding phase from described sintering temperature, is applied by described vertical column heating element heater (5) and to surpass 70% general power.
11. the described method of each claim is characterized in that as described above, described one or several pallets are enclosed in the column graphite rice steamers of being made up of three parts, and described three parts are rice steamer tube (2), rice steamer top board (3) and rice steamer base plate (4).
12. the described method of each claim as described above, it is characterized in that, described stove is in the situation of empty stove, and promptly in the situation without any pallet, the scope of the average natural cooldown rate drop to 1200 ℃ temperature range from 1400 ℃ is 9 ℃/minute to 14 ℃/minute.
13. the described method of each claim is characterized in that as described above, described stove and accessory has an extra thermocouple (16) of the centre that is positioned at the batch material, is used for before fast cooling step begins monitoring solidifying in the described bonding phase of described batch material.
14. a sintering furnace comprises: thermal insulation layer (9); Be positioned at least three independent controlled heating element heaters of described thermal insulation layer (9), described at least three independent controlled heating element heaters comprise and are fit to surround at least in part one or the vertical heating element heater (5) of several pallets, the lower horizontal heating element heater (7) that is arranged in the upper level heating element heater (6) on described stove top and is arranged in described stove bottom, wherein, described at least three heating element heaters can be operated and obtain 0.1 ℃/minute-4.0 ℃/minute average controlled cooldown rate.
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
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| SE0702911-9 | 2007-12-21 | ||
| SE0702911 | 2007-12-21 | ||
| PCT/SE2008/051525 WO2009082349A1 (en) | 2007-12-21 | 2008-12-19 | Sintering furnace and method of making cutting tools |
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| CN101903123A true CN101903123A (en) | 2010-12-01 |
| CN101903123B CN101903123B (en) | 2012-09-05 |
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|---|---|
| US (1) | US8889063B2 (en) |
| EP (1) | EP2225061B1 (en) |
| JP (1) | JP5603247B2 (en) |
| KR (1) | KR101520987B1 (en) |
| CN (1) | CN101903123B (en) |
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| CN107900330A (en) * | 2017-10-24 | 2018-04-13 | 嘉兴市鹏程磁钢有限公司 | A kind of magnet steel blank sintering equipment |
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| EP2821165A1 (en) * | 2013-07-03 | 2015-01-07 | Sandvik Intellectual Property AB | A sintered cermet or cemented carbide body and method of producing it |
| CN108253790A (en) * | 2018-04-01 | 2018-07-06 | 中鸿纳米纤维技术丹阳有限公司 | A kind of composite reinforcing material sintering furnace for the production of silica aerogel insulation quilt |
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| DE3625788A1 (en) * | 1986-07-30 | 1988-02-04 | Degussa | HIGH PRESSURE INTEROF |
| DE3883051T2 (en) * | 1987-04-24 | 1993-12-02 | Nippon Steel Corp | Process for the production of steel sheets with good toughness at low temperatures. |
| CA1319497C (en) * | 1988-04-12 | 1993-06-29 | Minoru Nakano | Surface-coated cemented carbide and a process for the production of the same |
| JPH03277701A (en) * | 1990-03-27 | 1991-12-09 | Mitsubishi Materials Corp | Method for sintering green compact using atmospheric sintering furnace |
| SE9003521D0 (en) | 1990-11-05 | 1990-11-05 | Sandvik Ab | HIGH PRESSURE ISOSTATIC DENSIFFICATION PROCESS |
| JP2910293B2 (en) | 1991-03-25 | 1999-06-23 | 三菱マテリアル株式会社 | Manufacturing method of tungsten carbide based cemented carbide cutting tool coated with hard layer |
| JPH05171442A (en) | 1991-12-25 | 1993-07-09 | Sumitomo Electric Ind Ltd | Coated sintered hard alloy and its manufacture |
| JPH05222404A (en) * | 1992-02-12 | 1993-08-31 | Daido Steel Co Ltd | Vacuum sintering furnace |
| SE505425C2 (en) * | 1992-12-18 | 1997-08-25 | Sandvik Ab | Carbide metal with binder phase enriched surface zone |
| US5414927A (en) * | 1993-03-30 | 1995-05-16 | Union Oil Co | Furnace elements made from graphite sheets |
| SE506482C2 (en) | 1996-04-23 | 1997-12-22 | Sandvik Ab | sintering Surface |
| JPH10141863A (en) * | 1996-11-07 | 1998-05-29 | Murata Mfg Co Ltd | Tubular furnace |
| JPH10281651A (en) | 1997-04-07 | 1998-10-23 | Fuji Oozx Inc | Method for heating work inside sintering furnace |
| JP3437427B2 (en) | 1997-12-04 | 2003-08-18 | 神鋼パンテツク株式会社 | Firing furnace for glass lining |
| US7019266B1 (en) * | 2001-07-20 | 2006-03-28 | Cape Simulations, Inc. | Substantially-uniform-temperature annealing |
| CN1541792B (en) | 2003-03-28 | 2012-05-09 | 三菱综合材料株式会社 | Method for manufacturing throwaway tip and apparatus for aligning green compact |
| JP2005002384A (en) | 2003-06-10 | 2005-01-06 | Hitachi Tool Engineering Ltd | Sintering method of cemented carbide |
| JP4888659B2 (en) * | 2007-10-03 | 2012-02-29 | 住友電工ハードメタル株式会社 | Replaceable cutting edge |
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| CN107900330A (en) * | 2017-10-24 | 2018-04-13 | 嘉兴市鹏程磁钢有限公司 | A kind of magnet steel blank sintering equipment |
| CN107900330B (en) * | 2017-10-24 | 2019-10-11 | 嘉兴市鹏程磁钢有限公司 | A kind of magnet steel blank sintering equipment |
Also Published As
| Publication number | Publication date |
|---|---|
| IL206244A0 (en) | 2010-12-30 |
| KR101520987B1 (en) | 2015-05-15 |
| US20110008199A1 (en) | 2011-01-13 |
| EP2225061A1 (en) | 2010-09-08 |
| JP5603247B2 (en) | 2014-10-08 |
| KR20100105616A (en) | 2010-09-29 |
| EP2225061A4 (en) | 2017-08-09 |
| JP2011508075A (en) | 2011-03-10 |
| EP2225061B1 (en) | 2019-04-24 |
| WO2009082349A1 (en) | 2009-07-02 |
| CN101903123B (en) | 2012-09-05 |
| US8889063B2 (en) | 2014-11-18 |
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